Cold water instant soft film softener and preparation method thereof

Abstract

The present invention discloses a cold-water instant film softener and a preparation method thereof. The cold-water instant film softener has the general structural formula: #imgabs0# and is prepared from N,N'-bis(2-hydroxyethyl)ethylenediamine, 12-hydroxystearic acid, methoxypolyethylene glycol glycidyl ether, and diethyl sulfate as raw materials. The film softener prepared using the preparation method provided by the present invention can be rapidly dispersed and dissolved in a normal temperature water environment, dissolving thoroughly without any residue, greatly improving the fabric processing rate and reducing energy consumption and processing costs. The treated fabric is soft and fluffy, has little effect on the fabric color, and does not suffer from yellowing, greatly improving the fabric's texture and added value. The preparation process is simple, highly controllable, and requires low production equipment. The production process does not emit pollutants, is safe and environmentally friendly, uses inexpensive and readily available raw materials, and is low in cost. The softener is suitable for industrial production.

Description

Technical Field

[0001] The invention relates to the technical field of textile hand finishing agents, in particular to a cold water instant soft sheet softener and a preparation method thereof. Background Art

[0002] During the pre-dyeing and finishing processes in the textile industry, natural waxes and oils on the fiber surface are removed, resulting in a loss of smoothness and increased friction between fibers. Furthermore, during the various processing steps from weaving to finishing, textile machinery and chemical additives (for example, during high-heat treatments such as scouring and bleaching during the dyeing and finishing process) damage chemical and natural fibers. These treatments / processes ultimately result in a rough, stiff feel and reduced wearability of the finished fabric.

[0003] In order to repair damaged fibers, give the fabric a soft and smooth feel, and improve the quality of the finished product, in addition to mechanical finishing methods (rubbing the fabric repeatedly under tension) to adjust the displacement of the fabric interlacing points to improve the fabric's soft feel, chemical finishing methods are often used. Among them, the use of additives to improve the fiber's softness, antistatic properties, and rewetting properties is an important chemical finishing method.

[0004] Fabric softeners are a type of dyeing and finishing auxiliaries that create a soft, comfortable feel to fabrics by reducing the coefficient of friction between fibers or between fibers and the human body. After forming a film on the fiber surface, the softener reduces the fiber's surface tension, allowing the fibers to stretch more easily. This results in a fluffy, fuller fabric with a soft feel. Therefore, fabric softeners are an important textile auxiliaries.

[0005] Currently, the softeners commonly used in the printing and dyeing industry include silicone emulsion softeners, film softeners, and wax emulsion softeners. Compared to the high price of silicone emulsions, film softeners are inexpensive and are therefore widely used in the post-printing and dyeing finishing process. Film softeners are primarily classified into two categories: cationic and nonionic. They are generally produced by reacting stearic acid with an organic amine (such as diethylenetriamine and hydroxyethylethylenediamine), followed by dehydration and condensation to form an amide, or by further dehydration and cyclization to form an imidazoline structure. Finally, the product is obtained through quaternization and acidification.

[0006] Currently, most film softeners require prolonged processing at high temperatures, increasing production costs and hindering efficiency, hindering energy conservation and emission reduction. Therefore, a cold-water instant softener with a simple preparation process, a fluffy and soft feel, and a simple, fast-acting, cold-water-soluble film softener and its preparation method are urgently needed. Such a film can quickly disperse and dissolve in ambient water, imparting various special features and styles to textiles, such as softness, wrinkle resistance, shrinkage resistance, waterproofing, antibacterial properties, and antistatic properties. It also saves energy and reduces processing costs, playing an indispensable role in improving the quality and added value of textiles. Summary of the Invention

[0007] The present invention aims to provide a cold-water instant film softener and a preparation method thereof, so as to simplify the preparation process of the film softener without affecting the use effect of the softener, reduce energy consumption and cost in the production process, and realize rapid dissolution in room temperature water / cold water.

[0008] To achieve the above object, the present invention provides a cold water instant soft film softener and a preparation method thereof. The cold water instant soft film softener has the general structural formula:

[0009]

[0010] Preferably, the cold water instant soft film softener is prepared from N,N'-bis(2-hydroxyethyl)ethylenediamine, 12-hydroxystearic acid, methoxy polyethylene glycol glycidyl ether and diethyl sulfate as raw materials; the molar ratio of N,N'-bis(2-hydroxyethyl)ethylenediamine:12-hydroxystearic acid:methoxy polyethylene glycol glycidyl ether:diethyl sulfate is 1:(1.0-1.5):(1.0-1.5):(1.0-1.5).

[0011] Preferably, the molar ratio of N,N'-bis(2-hydroxyethyl)ethylenediamine:12-hydroxystearic acid:methoxypolyethylene glycol glycidyl ether:diethyl sulfate is 1:(1.05-1.15):(1.05-1.15):(1.05-1.15).

[0012] Preferably, the molar ratio of N,N'-bis(2-hydroxyethyl)ethylenediamine:12-hydroxystearic acid:methoxypolyethylene glycol glycidyl ether:diethyl sulfate is 1:1.05:1.05:1.15.

[0013] Preferably, the methoxy polyethylene glycol glycidyl ether is one or more of methoxy polyethylene glycol 400 glycidyl ether, methoxy polyethylene glycol 600 glycidyl ether, and methoxy polyethylene glycol 800 glycidyl ether.

[0014] A method for preparing the above-mentioned cold water instant soft film softener comprises the following steps:

[0015] S1. Add 12-hydroxystearic acid and a catalyst to N,N'-bis(2-hydroxyethyl)ethylenediamine, stir evenly, and react for 2 to 4 hours at a certain temperature and vacuum conditions to obtain mono-12-hydroxystearic acid amide;

[0016] S2. Cooling the reaction system to 65-75° C., and reacting the mono-12-hydroxystearic acid amide obtained in step S1 with methoxy polyethylene glycol glycidyl ether for 5-7 hours;

[0017] S3, heating the reaction system to 80-90°C, adding diethyl sulfate to the product obtained in step S2, and keeping the temperature for 3-5 hours;

[0018] S4. The reaction product is adjusted to a pH of 6 to 8 with acetic acid, and the product is sliced to obtain a cold water instant soft sheet softener.

[0019] Preferably, the catalyst in step S1 is phosphorous acid; the certain temperature is 130 to 150° C., and the certain vacuum degree is -0.1 to -0.08 MPa.

[0020] Preferably, the amount of the catalyst added in step S1 is 0.5 to 1.5% of the total mass of N,N'-bis(2-hydroxyethyl)ethylenediamine and 12-hydroxystearic acid.

[0021] The invention relates to an application of the cold water instant soft sheet softener in fabric treatment.

[0022] By introducing a large number of hydrophilic groups (hydroxyl groups) and the water-soluble unit structure of polyethylene glycol into the product structure, the present invention achieves rapid dispersion and dissolution in water at room temperature, thereby reducing product energy consumption, improving production efficiency, and achieving energy conservation and emission reduction. Furthermore, the preparation method provided by the present invention does not contain environmentally prohibited components such as APEO. The resulting film softener is a quaternary ammonium salt-based cationic film, which provides a soft and fluffy feel, enhances the texture of textiles, and increases the added value of fabric products.

[0023] The present invention provides a cold water instant soft film softener and a preparation method thereof, and its specific technical effects are as follows:

[0024] 1. The film softener prepared by the preparation method provided by the present invention does not require long-term dissolution under high temperature conditions and can be quickly dispersed and dissolved in a normal temperature water environment. It dissolves completely without any residue, which can greatly improve the processing rate of fabrics and reduce energy consumption and processing costs.

[0025] 2. The fabric treated with the film softener prepared by the preparation method provided by the present invention is soft and fluffy, has little effect on the color of the fabric, and does not cause yellowing, which can greatly improve the texture and added value of the fabric;

[0026] 3. The preparation process provided by the present invention is simple, highly controllable, and has low requirements for production equipment; the production process does not emit pollutants, is safe and environmentally friendly; the raw materials used are cheap and easily available, and the cost is low; and it is suitable for industrial production.

[0027] The technical solution of the present invention is further described in detail below through examples. DETAILED DESCRIPTION

[0028] At present, most film softeners require long-term chemical reaction at high temperature, resulting in high energy consumption, complex preparation process, and low production efficiency. The present invention uses N,N'-bis(2-hydroxyethyl)ethylenediamine, 12-hydroxystearic acid, methoxy polyethylene glycol glycidyl ether, and diethyl sulfate as raw materials. Under a nitrogen atmosphere and with phosphorous acid as a catalyst, at 130-150°C, N,N'-bis(2-hydroxyethyl)ethylenediamine and 12-hydroxystearic acid are subjected to amidation reaction to form mono-12-hydroxystearic acid amide. The temperature is then lowered to 65-75°C, and methoxy polyethylene glycol glycidyl ether and 12-hydroxystearic acid monoamide are subjected to ring-opening addition reaction. Finally, the temperature is raised to 80-90°C, and diethyl sulfate is added for quaternization. Finally, a small amount of acetic acid is used to adjust the pH to 6-8, and the product is discharged and sliced to obtain a cold-water instant film softener. Its structural formula is:

[0029]

[0030] By introducing a large number of hydrophilic groups (hydroxyl groups) and the water-soluble unit structure of polyethylene glycol into the product structure, the present invention achieves rapid dispersion and dissolution in water at room temperature, thereby reducing product energy consumption, improving production efficiency, and achieving energy conservation and emission reduction. Furthermore, the preparation method provided by the present invention does not contain environmentally prohibited components such as APEO. The resulting film softener is a quaternary ammonium salt-based cationic film, which provides a soft and fluffy feel, enhances the texture of textiles, and increases the added value of fabric products.

[0031] The technical solution of the present invention is further illustrated by the following examples.

[0032] In order to make the purpose, technical solutions and advantages of the present application clearer, more thorough and more complete, the technical solutions in the embodiments of the present invention are clearly and completely described below by way of examples. The following detailed description is the description of the embodiments, and is intended to provide further details of the present invention. Unless otherwise indicated, all technical terms used in the present invention have the same meaning as that generally understood by those of ordinary skill in the art to which the application belongs.

[0033] The reagents and instruments used in the examples were obtained from commercial sources.

[0034] Example 1

[0035] A cold water instant softener is prepared as follows:

[0036] S1. Add 315.5 g of 12-hydroxystearic acid and 2.3 g of phosphorous acid to 150.0 g of N,N'-bis(2-hydroxyethyl)ethylenediamine, stir evenly, and react at 130° C. and a vacuum degree of -0.08 MPa for 4 h to obtain mono-12-hydroxystearic acid amide;

[0037] S2. Cool the reaction system to 65° C. and react the mono-12-hydroxystearic acid amide obtained in step S1 with 473.0 g of methoxy polyethylene glycol 400 glycidyl ether for 7 h;

[0038] S3, heating the reaction system to 80°C, adding 177.0 g of diethyl sulfate to the product obtained in step S2, and keeping the temperature for 5 hours;

[0039] S4. The reaction product is adjusted to pH 6 with acetic acid, and the product is sliced to obtain a cold water instant soft sheet softener.

[0040] Example 2

[0041] A cold water instant softener is prepared as follows:

[0042] S1. Add 330.5 g of 12-hydroxystearic acid and 4.8 g of phosphorous acid to 150.0 g of N,N'-bis(2-hydroxyethyl)ethylenediamine, stir evenly, and react at 140° C. and a vacuum degree of -0.09 MPa for 3 h to obtain mono-12-hydroxystearic acid amide;

[0043] S2. Cool the reaction system to 70° C. and react the mono-12-hydroxystearic acid amide obtained in step S1 with 715.0 g of methoxy polyethylene glycol 600 glycidyl ether for 6 h;

[0044] S3, heating the reaction system to 85°C, adding 169.6 g of diethyl sulfate to the product obtained in step S2, and keeping the temperature for 4 hours;

[0045] S4. The reaction product is adjusted to pH 7 with acetic acid, and the product is sliced to obtain a cold water instant soft sheet softener.

[0046] Example 3

[0047] A cold water instant softener is prepared as follows:

[0048] S1. Add 345.5 g of 12-hydroxystearic acid and 7.4 g of phosphorous acid to 150.0 g of N,N'-bis(2-hydroxyethyl)ethylenediamine, stir evenly, and react at 150° C. and a vacuum degree of -0.1 MPa for 2 h to obtain mono-12-hydroxystearic acid amide;

[0049] S2. Cool the reaction system to 75° C. and react the mono-12-hydroxystearic acid amide obtained in step S1 with 977.5 g of methoxy polyethylene glycol 800 glycidyl ether for 5 h;

[0050] S3, heating the reaction system to 90°C, adding 161.9 g of diethyl sulfate to the product obtained in step S2, and keeping the temperature for 3 hours;

[0051] S4. The reaction product is adjusted to pH 8 with acetic acid, and the product is sliced to obtain a cold water instant soft sheet softener.

[0052] Effect Example 1

[0053] Take the samples of Examples 1, 2, and 3 and 50 g of commercially available cationic film S500 respectively and add them to 450 mL of room temperature water (diluted at 1:9), stir them at a fixed speed of 100 r / min for 10 min with a stirrer of the same specifications, and then filter them with a 120-mesh filter to compare the water solubility of the dispersions. The results are shown in Table 1.

[0054] Effect Example 2

[0055] Take 50g of the 1:9 thin film in Example 1 and add it to 1L of water as the working solution. The 15×20cm cotton and white woven fabrics of the same material are treated with the padding process: two dips and two pads (liquid rate 65%) → drying → shaping (160℃×60s) → regain 3h → comparative test of the feel and whiteness of the finished fabrics. The results are shown in Table 1.

[0056] The commercially available cationic film S500 was used to prepare the working solution using the method in the instructions, and then the same padding process as above was used for padding treatment. The test results are shown in Table 1.

[0057] The hand feel is determined by the average of five people's evaluations, with 5 being the highest and 1 being the lowest. A higher score indicates a softer and fluffier feel, while a lower score indicates a worse feel.

[0058] Whiteness is measured using a whiteness meter, with the average value calculated from ten measurements taken at different locations. Higher whiteness values indicate less yellowing and discoloration, and less impact of the softener on the color shade of the dyed fabric. See Table 1 for the results.

[0059] Table 1

[0060] film Filter results feel Whiteness Example 1 No residue 4.7 98.5 Example 2 No residue 4.9 98.2 Example 3 No residue 5 98.8 S500 cationic film More lumps 4.5 98.3

[0061] Result Analysis

[0062] As can be seen from the data in Table 1, the feel and whiteness of the cold-water instant-soluble films prepared in Examples 1 and 3 of the present invention are slightly better than those of the commercially available S500 cationic film. The fabric treated with the film prepared in Example 3 has the best feel and whiteness, with a perfect feel score and a whiteness value of 98.8. The films prepared in Examples 1 to 3 are significantly better in cold water dispersibility and dissolution rate than the commercially available S500 cationic film.

[0063] Therefore, the film softener prepared by the preparation method provided by the present invention can be quickly dispersed and dissolved in a normal temperature water environment, dissolves completely without any residue, can greatly improve the processing rate of fabrics, reduce energy consumption and processing costs; the treated fabrics are soft and fluffy, have little effect on the color of the fabrics, and no yellowing occurs, which can greatly improve the texture and added value of the fabrics; the preparation process is simple, controllable, and has low requirements for production equipment; the production process does not emit pollutants, is safe and environmentally friendly; the raw materials used are cheap and easily available, and the cost is low; and the process is suitable for industrial production.

[0064] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the same. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that they can still modify or replace the technical solutions of the present invention with equivalents, and these modifications or equivalent replacements cannot cause the modified technical solutions to deviate from the spirit and scope of the technical solutions of the present invention.

Claims

1. A cold water instant soft film softener, characterized in that: The general structural formula of the cold water instant soft film softener is:

2. The cold water instant softener according to claim 1, characterized in that: The invention is prepared from N,N'-bis(2-hydroxyethyl)ethylenediamine, 12-hydroxystearic acid, methoxy polyethylene glycol glycidyl ether and diethyl sulfate as raw materials; the molar ratio of N,N'-bis(2-hydroxyethyl)ethylenediamine:12-hydroxystearic acid:methoxy polyethylene glycol glycidyl ether:diethyl sulfate is 1:(1.0-1.5):(1.0-1.5):(1.0-1.5).

3. The cold water instant softener according to claim 2, characterized in that: The molar ratio of N,N'-bis(2-hydroxyethyl)ethylenediamine:12-hydroxystearic acid:methoxypolyethylene glycol glycidyl ether:diethyl sulfate is 1:(1.05-1.15):(1.05-1.15):(1.05-1.15).

4. The cold water instant softener according to claim 2, characterized in that: The molar ratio of N,N'-bis(2-hydroxyethyl)ethylenediamine:12-hydroxystearic acid:methoxypolyethylene glycol glycidyl ether:diethyl sulfate is 1:1.05:1.05:1.

15.

5. The cold water instant softener according to claim 2, characterized in that: The methoxy polyethylene glycol glycidyl ether is one or more of methoxy polyethylene glycol 400 glycidyl ether, methoxy polyethylene glycol 600 glycidyl ether, and methoxy polyethylene glycol 800 glycidyl ether.

6. A method for preparing the cold water instant softener according to any one of claims 1 to 5, characterized in that: The following steps are involved: S1. Add 12-hydroxystearic acid and a catalyst to N,N'-bis(2-hydroxyethyl)ethylenediamine, stir evenly, and react for 2 to 4 hours at a certain temperature and vacuum conditions to obtain mono-12-hydroxystearic acid amide; S2. Cooling the reaction system to 65-75° C., and reacting the mono-12-hydroxystearic acid amide obtained in step S1 with methoxy polyethylene glycol glycidyl ether for 5-7 hours; S3, heating the reaction system to 80-90°C, adding diethyl sulfate to the product obtained in step S2, and keeping the temperature for 3-5 hours; S4. The reaction product is adjusted to a pH of 6 to 8 with acetic acid, and the product is sliced to obtain a cold water instant soft sheet softener.

7. The method for preparing a cold water instant softener according to claim 6, wherein: The catalyst in step S1 is phosphorous acid; the certain temperature is 130 to 150° C., and the certain vacuum degree is -0.1 to -0.08 MPa.

8. The method for preparing a cold water instant softener according to claim 6, wherein: The amount of the catalyst added in step S1 is 0.5-1.5% of the total mass of N,N'-bis(2-hydroxyethyl)ethylenediamine and 12-hydroxystearic acid.

9. Use of the cold water instant softener according to any one of claims 1 to 5 in textile processing.

Images